EP0757665B1 - Verfahren zur herstellung eines cristobalit enthaltenden quarzglases - Google Patents

Verfahren zur herstellung eines cristobalit enthaltenden quarzglases Download PDF

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Publication number
EP0757665B1
EP0757665B1 EP96903002A EP96903002A EP0757665B1 EP 0757665 B1 EP0757665 B1 EP 0757665B1 EP 96903002 A EP96903002 A EP 96903002A EP 96903002 A EP96903002 A EP 96903002A EP 0757665 B1 EP0757665 B1 EP 0757665B1
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EP
European Patent Office
Prior art keywords
silica glass
cristobalite
containing silica
mixture
temperature
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP96903002A
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English (en)
French (fr)
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EP0757665A1 (de
Inventor
Kyoichi Inaki
Tohru Segawa
Nobumasa Yoshida
Mamoru Endo
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Heraeus Quarzglas GmbH and Co KG
Shin Etsu Quartz Products Co Ltd
Original Assignee
Heraeus Quarzglas GmbH and Co KG
Shin Etsu Quartz Products Co Ltd
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Filing date
Publication date
Priority claimed from JP09749495A external-priority patent/JP3400180B2/ja
Application filed by Heraeus Quarzglas GmbH and Co KG, Shin Etsu Quartz Products Co Ltd filed Critical Heraeus Quarzglas GmbH and Co KG
Priority to EP98105181A priority Critical patent/EP0854116B1/de
Publication of EP0757665A1 publication Critical patent/EP0757665A1/de
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Publication of EP0757665B1 publication Critical patent/EP0757665B1/de
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C14/00—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix
    • C03C14/004—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix the non-glass component being in the form of particles or flakes
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B20/00—Processes specially adapted for the production of quartz or fused silica articles, not otherwise provided for
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B32/00—Thermal after-treatment of glass products not provided for in groups C03B19/00, C03B25/00 - C03B31/00 or C03B37/00, e.g. crystallisation, eliminating gas inclusions or other impurities; Hot-pressing vitrified, non-porous, shaped glass products
    • C03B32/02—Thermal crystallisation, e.g. for crystallising glass bodies into glass-ceramic articles
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/06—Glass compositions containing silica with more than 90% silica by weight, e.g. quartz
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2201/00—Glass compositions
    • C03C2201/02—Pure silica glass, e.g. pure fused quartz
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2201/00—Glass compositions
    • C03C2201/80—Glass compositions containing bubbles or microbubbles, e.g. opaque quartz glass
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2214/00—Nature of the non-vitreous component
    • C03C2214/20—Glass-ceramics matrix
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2214/00—Nature of the non-vitreous component
    • C03C2214/30—Methods of making the composites

Definitions

  • the present invention relates to a method of producing a cristobalite-containing silica glass. More particularly, it relates to a method of producing the ⁇ -cristobalite-containing silica glass having ⁇ -cristobalite in the shape of a small sphere or a small, round-edged or sharp-edged, three-dimensional region dispersed in the silica glass matrix.
  • Silica glass has been heretofore used in fields such as of a jig for use in semiconductor device fabrication and the like wherein high purity, heat-resistance and chemical resistance are required, since silica glass is generally good in heat-resistance, chemical resistance and further good in processability and cleanablity.
  • the crystal-containing silica glass proposed in the Journal of the American Ceramic Society mentioned above uses a crystal forming agent to form a crystal phase in the silica glass matrix, it has a fault that the crystal forming agent out-diffuses impurities to thereby contaminate a semiconductor device being fabricated, when the jig is used in a temperature higher than 1000 °C.
  • a silica glass jig the surface of which is covered with a vapor deposited thin film made of metal or ceramic thereon, has been proposed, but since the thermal expansion coefficient of silica glass is usually smaller than those of the metal or ceramic, the thin film contracts to a great extent and thereby has a problem that a crack occurs in the thin film when it is used in a high temperature treatment of a silicon wafer. This problem has blocked the practical application of a thin film on the surface of a jig.
  • a refractory material which contains amorphous silica as well as 45 - 60 wt.% of a crystalline phase of silica.
  • the refractory material is made by mixing powders of amorphous and crystalline powders, whereby the particles dimensions are between 75 ⁇ m and 150 ⁇ m and sintering the mixture.
  • JP-A 1 126 238 as interpreted by a PAJ-abstract describes a silica glass member containing cristobalite. Cristobalite crystals having sizes between 5 ⁇ m and 1000 ⁇ m are obtained by growing strain seeds which are formed in the glass matrix.
  • a ceramic moulding consisting of quartz sand, cristobalite and alkali-alkaline earth-alumino borosilicate glass.
  • JP-A 62 202 826 as interpreted by a PAJ-abstract describes a method for producing high-quality glass at low cost, by mixing SiO 2 -powder with a phase transition promotor, heat treating to achieve a growing of cristobalite crystals and melting the crystalline phase in vacuum to obtain a high quality transparent or functional glass.
  • silica glass having the characteristics above mentioned can be produced by incorporating ⁇ -crystobalite in the shape of a small sphere or a small, round-edged or sharp-edged, three-dimensional region dispersed in the bulk of silica glass matrix and further the silica glass with a lower light transmission is obtained by dispersing small-sized independent bubbles at a content in a range in the matrix as compared with that of the silica glass with no independent bubbles.
  • the present inventors have also discovered a fact that the silica glass with all the characteristics mentioned above can be produced with ease by heating to melt a mixture of two or more kinds of crystalline silicon dioxide powder which have different melting points from each other by 20 °C or more at a temperature in a range.
  • the present invention has been completed on the basis of such knowledge as mentioned above.
  • the present invention is directed to a method of producing a cristobalite-contained silica glass according to claim 1. Further embodiments of the invention are defined in the dependent claims.
  • the cristobalite-containing silica glass produced according to the present invention has ⁇ -crystobalite in the shape of a small sphere or a small, round-edged or sharp-edged, three-dimensional region dispersed in the silica glass matrix, a diameter of each small sphere or region is in the range of 0.1 ⁇ m to 1000 ⁇ m and a content of the cristobalite is in the range of 10 wt % to 99 wt %.
  • the thermal expansion coefficient of silica glass is increased by containing the cistobalite phase in the matrix and can be adjusted to a value equal to or larger than 1 x 10 -6 /°C which is a thermal expansion coefficient of a vapor-deposited film formed in a chemical vapor deposition process.
  • 1 x 10 -6 /°C is a thermal expansion coefficient of a vapor-deposited film formed in a chemical vapor deposition process.
  • the ⁇ -cristobalite-containing silica glass according to the present invention is produced by heating to melt a mixture of two or more kinds crystalline silicon dioxide powder the melting points of which are different from each other by 20 °C or more, with a content of ⁇ -cristobalite more than 80 wt %, cracks usually occur in a body of the ⁇ -cristobalite-containing silica glass, but even with a content of ⁇ -cristobalite of 99 wt %, it is possible that cracks do not occur in a body of the ⁇ -cristobalite-containing silica glass, if it is re-heated at a temperature of 1000 °C or higher and thereby a crystal of ⁇ -cristobalite is gradually grown.
  • the re-heating time changes in dependence on a content of ⁇ -cristobalite.
  • a content of the silicon dioxidepowder having the highest melting point in the mixture is larger, the re-heating time can be decreased and vice versa.
  • Any atmosphere can be chosen in the heat treatment.
  • the cristobalite-containing silica glass becomes opaque due to the presence of crystobalite phase in the matrix, for cracks are generated between a crystal of cristobalite and the silica glass matrix and the cracks scatter incident rays.
  • a diameter of each bubble dispersed in the matrix is preferably 500 ⁇ m or smaller and a concentration is preferably in the range of 100 bubbles/cm 3 to 100.000 bubbles/cm 3 .
  • the cristobalite-containing silica glass which, in addition to the above characteristics, has a density of 2.0 g/cm 3 or more and a three-point bending strength of 150 kg/cm 2 or more can be effectively used as a material of a jig for use in semiconductor device fabrication.
  • the light transmission can be reduced to a smaller value by re-heating to grow a crystal of ⁇ -cristobalite to an greater degree and it can be adjusted to a value of 1 % or less. It is possible to manufacture a jig such as an excellent heat-ray scattering member from the crystal-containing silica glass with such a low light transmission as this.
  • a content of independent bubbles in the matrix can be lowered to a value of the order of one tenth in comparison with that of a traditional opaque quartz glass, while the degree of opaqueness is still better than that of the traditional opaque quartz glass.
  • the cristobalite-containing silica glass is produced in the following steps of first charging a raw material mixture of two or more kinds of crystalline silicon dioxide powder the melting points of which are different from each other by 20 °C or more, the silicon dioxide powder having the highest melting point of which is mixed at a content of 10 wt % to 80 wt %, and a particle size of each powder is in the range of 10 ⁇ m to 1000 ⁇ m in a heat resistant mold, and second heating the mold and the charged mixture at a temperature between the lowest melting point and a temperature less than the highest melting point of the ingredients of the mixture.
  • the mixture is heated at a first heating speed of 10 °C/min to 50 °C/min from room temperature to 1000 °C, secondly at a second heating speed of 10 °C/min or lower from the 1000 °C up to a first temperature in the range of the lowest melting point to a second temperature of 10 °C higher than the lowest melting point, thirdly slowly from the first temperature up to a third temperature lower than the highest melting temperature, and fourthly the mixture is constantly kept at the third temperature.
  • ⁇ -quartz is used as crystalline silicon dioxide and the structural form of ⁇ -quartz transits to ⁇ -quartz, ⁇ -tridymite and to ⁇ -cristobalite when heating to melt it and if the ⁇ -cristobalite is heated at a temperature of the melting point or higher, the crystal changes into a liquid to be in a vitrified state.
  • Silica glass is obtained by cooling down the ⁇ -cristobalite in the vitrified state to room temperature to reach a supercooled condition.
  • the melting point of ⁇ -cristobalite is 1723 °C according to a technical document.
  • the silicon dioxide powder having the lowest melting point is first molten to form a silica glass matrix and on the other hand the silicon dioxide powder having the highest melting point remains unmelted to form cristobalite regions.
  • crystal-containing silica glass contains neither impurities such as a crystal forming agent nor gaps formed by sintering and thereby is high both in purity and in mechanical strength, since it is produced by neither sintering nor doping a crystal forming agent.
  • the structural form of ⁇ -cristobalite is one form of SiO 2 crystal. A fact that the size of a crystal region is smaller than the size of each particle of the crystalline silicon dioxide powder having the highest melting point seemingly comes from a cause that particles of the crystalline silicon dioxide powder are further pulverized to smaller sizes in a vitrification process.
  • a carbon-made mold, a ceramic-made mold and a transparent quartz tube inserted in the molds just mentioned are named as heat resistant molds for use in charging a mixture of crystalline silicon dioxide powder.
  • a transparent quartz tube high purity of the raw material charged can be maintained and at the same time silica glass produced does not have a chance for the bulk form to collapse.
  • a transparent quartz tube as a mold is excellent.
  • An electric-melting method is adopted as a heating means for melting, since it has a little chance for OH groups to mixed in silica glass, and thereby the silica glass being highly heat-resistant is produced.
  • an inert gas atmosphere such as a nitrogen atmosphere or a vacuum atmosphere is generally used.
  • an inert gas atmosphere is specially required.
  • a gas in the atmosphere is not so much specialized.
  • the powder mixture was charged in a silica glass tube inserted in a carbon made mold, then the air lying in the gaps between the particles of the powder mixture was removed by vacuum suction. After completion of air removal, the space in the silica glass tube was filled with nitrogen gas. In the nitrogen atmosphere the powder mixture was heated from room temperature to 1000 °C in 90 min, from the 1000 °C to 1200 °C in 30 min, from the 1200 °C to 1630 °C in 90 min, and from the 1630 °C to 1720 °C in 180 min and then kept at a constant temperature of the 1720 °C for 1 h. The powder mixture thus treated became cristobalite-containing silica glass.
  • ⁇ -cristobalite in the shape of a small sphere of about 40 ⁇ m in diameter was observed at a content of 30 wt % in the silica glass matrix.
  • Observation by an electron microscope was schematically drawn in Fig. 2 to show the feature thereof.
  • the sizes of crystalline regions, thermal expansion coefficient, light transmission, and bending strength were measured on samples of the cristobalite-containing silica glass and the results are shown in Table 1.
  • the measurement of x ray diffraction is shown in Chart 1 and from the chart, the structural form of the crystal regions was identified as ⁇ -cristobalite, as shown in Chart 1.
  • the cristobalite-containing silica glass produced in Example 1 was further heated at 1400 °C for 60 h.
  • An ⁇ -cristobalite region had grown to that of about 100 ⁇ m in diameter.
  • Observation by the electron microscope is schematically shown in Fig. 3.
  • the sizes of the cristobalite regions and the thermal expansion coefficient, light transmission, and bending strength of the cristobalite-containing silica glass were measured and the results are shown in Table 1.
  • the structural form of a crystal zone in the silica glass matrix was identified as ⁇ -cristobalite by the x ray diffraction analyzer.
  • Cristobalite-containing silica glass was produced in the same way as in Example 1 with an exception that a mixture of crystalline silicon dioxide powder was prepared from Iota CGU Fine and Iota 6 Fine at a ratio of 50:50.
  • the sizes of cristobalite regions and thermal expansion coefficient, light transmission, and bending strength of the cristobalite-containing silica glass thus produced were measured and the results are shown in Table 1.
  • the structural form of a crystal region in the silica glass matrix was identified as ⁇ -cristobalite by the x ray diffraction analyzer.
  • the cristobalite-containing silica glass produced in Example 3 was further heated at 1400 °C for 20 h.
  • An ⁇ -cristobalite region had grown to that of about 100 ⁇ m in diameter.
  • the sizes of the cristobalite regions and the thermal expansion coefficient, light transmission, and bending strength of the cristobalite-containing silica glass thus produced were measured and the results are shown in Table 1.
  • the structural form of a crystal region in the silica glass matrix was identified as ⁇ -cristobalite by the x ray diffraction analyzer.
  • Cristobalite-containing silica glass was produced in the same way as in Example 1 with an exception that the powder mixture was molten in an atmosphere in which nitrogen gas flew at a rate of 10 l/min.
  • the powder mixture was molten in an atmosphere in which nitrogen gas flew at a rate of 10 l/min.
  • the matrix of the produced cristobalite-containing silica glass independent bubbles of diameters of 160 ⁇ m or smaller were observed at a concentration of 68.000 bubbles/cm 3 and the density was measured at 2.115 g/cm 3 .
  • the sizes of cristobalite regions and the thermal expansion coefficient, light transmission, and bending strength of the cristobalite-containing silica glass thus produced were measured and the results are shown in Table 1.
  • the structural form of a crystal region in the silica glass matrix was identified as ⁇ -cristobalite by the x ray diffraction analyzer.
  • Iota CGU Fine produced by Unimin Corporation was charged in a silica glass tube inserted in a carbon made mold and the powder was heated in a nitrogen atmosphere from room temperature to 1000 °C in 90 min, from the 1000 °C to 1200 °C in 30 min, from the 1200 °C to 1630 °C in 90 min, and from the 1630 °C to 1720 °C in 180 min and kept at a constant temperature of the 1720 °C for 1 h.
  • the powder thus treated became opaque silica glass.
  • the thermal expansion coefficient, light transmission, and bending strength of the opaque silica glass thus produced were measured and the results are shown in Table 1. Non-existence of a crystalline region in the silica glass matrix was confirmed as a result of an x ray diffraction analysis. A rocking curve obtained is shown in Chart 2.
  • Iota 6 Fine produced by Unimin Corporation was charged in a silica glass tube inserted in a carbon made mold and the powder was heated in a nitrogen atmosphere from room temperature to 1000 °C in 90 min, from the 1000 °C to 1200 °C in 30 min, from the 1200 °C to 1630 °C in 90 min, and from the 1630 °C to 1720 °C in 180 min and kept at a constant temperature of the 1720 °C for 1 h.
  • the powder thus treated became opaque silica glass.
  • the thermal expansion coefficient, light transmission, and bending strength of the opaque silica glass thus produced were measured and the results are shown in Table 1. Non-existence of a crystalline region in the silica glass matrix was confirmed as a result of an x ray diffraction analysis.
  • Example 1 Example 2 Example 3 Example 4 Example 5 Size of Crystal ( ⁇ m) 40 100 40 500 40 Thermal Expansion Coefficient (Average RT ⁇ 700 °C) 1 X 10 -6 3 X 10 -6 1 X 10 -6 10 X 10 -6 1 X 10 -6 Transmittance at 2 ⁇ m 1.0 0.3 0.5 0.1 0.5 Bending Strength (kg/cm 2 ) 350 200 250 150 250 Com Ex 1 Com Ex 2 Com Ex 3 Size of Crystal ( ⁇ m) none none none Thermal Expansion Coefficient (Average RT ⁇ 700 °C) 5 X 10 -7 5 X 10 -7 5 X 10 -7 Transmittance at 2 ⁇ m 8 5 80 Bending Strength (kg/cm 2 ) 500 500 550

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Claims (4)

  1. Verfahren zur Herstellung von Cristobalit enthaltendem Quarzglas, dadurch gekennzeichnet, daß zwei oder mehr Arten kristallinen Siliziumoxid-Pulvers, dessen Schmelzpunkte um 20°C oder mehr differieren, zur Herstellung eines Gemisches verwendet werden, wobei der Gehalt an Siliziumoxid mit dem höchsten Schmelzpunkt 10 Gew.-% bis 80 Gew.-% beträgt und die Erhitzungstemperatur des Gemisches zwischen dem niedrigsten und dem höchsten Schmelzpunkt der Inhaltsstoffe liegt.
  2. Verfahren zur Herstellung von Cristobalit enthaltendem Quarzglas nach Anspruch 1, dadurch gekennzeichnet, daß das Gemisch mit einer ersten Aufheizgeschwindigkeit im Bereich zwischen 10°C/min und 50°C/min von Raumtemperatur bis auf 1000°C erhitzt wird und mit einer zweiten Aufheizgeschwindigkeit von 10°C/min oder weniger von 1000°C bis auf eine Temperatur zwischen dem niedrigsten Schmelzpunkt der Inhaltsstoffe und 10°C oberhalb des niedrigsten Schmelzpunktes erhitzt wird, und daß ein weiteres Erhitzen mit einer dritten geringen Aufheizgeschwindigkeit bis auf eine Temperatur unterhalb des höchsten Schmelzpunktes der Inhaltsstoffe erfolgt.
  3. Verfahren zur Herstellung von Cristobalit enthaltendem Quarzglas nach Anspruch 1 oder 2, dadurch gekennzeichnet, daß der Partikeldurchmesser des kristallinen Siliziumoxid-Pulvers im Bereich zwischen 10 µm und 1000 µm liegt.
  4. Verfahren zur Herstellung von Cristobalit enthaltendem Quarzglas nach Anspruch 1 oder 2, dadurch gekennzeichnet, daß das Gemisch in einer Stickstoffatmosphäre mit einer Flußrate im Bereich zwischen 5 l/min und 20 l/min erhitzt wird, so daß kleine einzeln vorliegende Blasen dispergiert in der Quarzglas-Matrix erhalten werden.
EP96903002A 1995-02-28 1996-02-27 Verfahren zur herstellung eines cristobalit enthaltenden quarzglases Expired - Lifetime EP0757665B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP98105181A EP0854116B1 (de) 1995-02-28 1996-02-27 Cristobalit enthaltendes Quarzglas, und daraus hergestellte Quarzglas-Haltevorrichtung

Applications Claiming Priority (5)

Application Number Priority Date Filing Date Title
JP6487695 1995-02-28
JP64876/95 1995-02-28
JP09749495A JP3400180B2 (ja) 1995-03-31 1995-03-31 シリカガラス治具
JP97494/95 1995-03-31
PCT/EP1996/000794 WO1996026908A1 (en) 1995-02-28 1996-02-27 Cristobalite-contained silica glass, method of producing same and silica glass jig made of same

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EP98105181A Division EP0854116B1 (de) 1995-02-28 1996-02-27 Cristobalit enthaltendes Quarzglas, und daraus hergestellte Quarzglas-Haltevorrichtung

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EP0757665A1 EP0757665A1 (de) 1997-02-12
EP0757665B1 true EP0757665B1 (de) 1998-10-14

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EP98105181A Expired - Lifetime EP0854116B1 (de) 1995-02-28 1996-02-27 Cristobalit enthaltendes Quarzglas, und daraus hergestellte Quarzglas-Haltevorrichtung
EP96903002A Expired - Lifetime EP0757665B1 (de) 1995-02-28 1996-02-27 Verfahren zur herstellung eines cristobalit enthaltenden quarzglases

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US (1) US5876473A (de)
EP (2) EP0854116B1 (de)
KR (1) KR100197471B1 (de)
DE (2) DE69611686T2 (de)
TW (1) TW382007B (de)
WO (1) WO1996026908A1 (de)

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JP3970692B2 (ja) * 2002-05-31 2007-09-05 信越化学工業株式会社 プリフォーム製造方法
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JPS62202826A (ja) * 1986-02-28 1987-09-07 Nippon Sanso Kk ガラスの製造法
JPH01126238A (ja) * 1987-11-09 1989-05-18 Shinetsu Sekiei Kk 石英ガラス炉芯管
US4935046A (en) * 1987-12-03 1990-06-19 Shin-Etsu Handotai Company, Limited Manufacture of a quartz glass vessel for the growth of single crystal semiconductor

Also Published As

Publication number Publication date
EP0854116A2 (de) 1998-07-22
DE69611686D1 (de) 2001-03-01
KR960031363A (ko) 1996-09-17
DE69600781D1 (de) 1998-11-19
US5876473A (en) 1999-03-02
EP0854116B1 (de) 2001-01-24
KR100197471B1 (ko) 1999-06-15
EP0757665A1 (de) 1997-02-12
TW382007B (en) 2000-02-11
DE69611686T2 (de) 2001-08-02
WO1996026908A1 (en) 1996-09-06
DE69600781T2 (de) 1999-05-20
EP0854116A3 (de) 1999-01-07

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